Preparation of cellulose nanoparticles from agave waste and its morphological and structural characterization

Preparación de nanopartículas de celulosa a partir de desechos de agave y su caracterización morfológica y estructural

C.E. Ponce-Reyes¹, J.J. Chanona-Pérez¹*, V. Garibay-Febles², E. Palacios-González², J. Karamath², E. Terrés-Rojas², G. Calderón-Domínguez¹

¹ Departamento de Ingeniería Bioquímica, Prolongación de Carpió y Plan de Ayala s/n, (Col. Santo Tomas C.P. 11340 Miguel Hidalgo. Escuela Nacional de Ciencias Biológicas, Instituto Politécnico Nacional. México, D.F. * Corresponding author. E-mail: jorge_chanona@hotmail.com.

² Laboratorio de Microscopia de Ultra Alta Resolución, Eje Central Lázaro Cárdenas Norte 152 Col. San Bartolo Atepehuacan C.P 07730) (Gustavo A. Madero. Instituto Mexicano del Petróleo. México, D.F.

Received May 9, 2014.
Accepted June 20, 2014.

Abstract

Agave is a natural waste from many different industries in Mexico, so alternative uses for these fibrous waste materials are desirable. Cellulose nanoparticles were obtained from dried agave leaves by acid hydrolysis. The characterization of the nanoparticles was made using scanning electron microscopy (SEM), Fast Fourier transformation infrared (FTIR) solid state nuclear magnetic resonance (ssNMR), X-ray diffraction (XRD) and high resolution transmission electron microscopy (HR-TEM). The nanoparticles had an average size of 97 ± 30 nm within a range of 31-198 nm, with a quasi-spherical and polyhedral morphology associated to a shape factor of 0.78 ± 0.06. The FTIR results revealed that the cellulose nanoparticles showed the characteristic cellulose peaks. Meanwhile, ssNMR showed the main peaks of the cellulose there was a difference in the peaks presence and absence when comparing to the cellulose pattern, which was associated to a lower crystallinity of the agave nanoparticles. In addition, the nanoparticles had a triclinic crystalline structure and a crystallinity index of 39% confirmed by HR-TEM and XRD. This study is important for a facile obtention of green nanomaterials from agroindustrial waste.

Keywords: agave waste, cellulose nanoparticles, crystallinity, microscopy, spectroscopy.

Resumen

El agave es un deshecho natural de diferentes industrias de México, por lo tanto, los usos alternativos de estos deshechos fibrosos son deseables. Nanopartículas de celulosa fueron producidas desde hojas de agave deshidratadas por hidrolisis acida. La caracterización de estas nanopartículas se llevo a cabo mediante microscopia electrónica de barrido (SEM), espectroscopia infrarroja con transformada de Fourier (FTIR), difracción de rayos X (XRD), resonancia magnética nuclear de estado sólido (ssNMR) y microscopia electrónica de transmisión de alta resolución (HRTEM). Las nanopartículas tuvieron un tamaño promedio de 97 ± 30 nm en un intervalo entre 31-198 nm y con morfología cuasi-esférica y poliédrica asociado a un factor de forma de 0.78 ± 0.06. Los resultados de la FTIR revelaron que las nanopartículas poseen los picos característicos de la celulosa, mientras que el espectro de ssNMR confirmo su naturaleza celulósica. Sin embargo, hubo diferencia en la presencia de picos en comparación con el espectro de la celulosa patrón, que fue asociado a una menor cristalinidad de las nanopartículas de agave. Además, las nanopartículas tuvieron una estructura cristalina triclínica y un índice de cristalinidad del 39 %, lo cual fue establecido mediante HRTEM y XRD. Este estudio es importante para la fácil obtención de nanomateriales verdes desde residuos agroindustriales.

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Acknowledgements

Claudia Ericka Ponce Reyes wishes to thank CONACYT for the scholarship provided for her studies and international stay. This research was funded through projects 20110627 and 20121001, 20130333 and 20140387 at the Instituto Politécnico Nacional (SIP-IPN México) and133102 of CONACYT.

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